Development and Validation of Novel GC-FID Method for Simultaneous Quantification of Paracetamol and Caffeine in Formulations

2020 ◽  
Vol 42 (4) ◽  
pp. 581-581
Author(s):  
Imtiaz Hussain Imtiaz Hussain ◽  
Yawar Baig Yawar Baig ◽  
Sara Naveed Sara Naveed ◽  
Muhammad Imran Khan Muhammad Imran Khan ◽  
Hafiz Shoaib Sarwar Hafiz Shoaib Sarwar ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Analytical Techniques ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Ich Guidelines ◽  
Highly Sensitive ◽  
Sensitivity And Selectivity ◽  
Development And Validation ◽  
Accurate Quantification

The advancements in analytical techniques have enabled the development of highly sensitive and accurate methods for the identification of materials up to trace levels using microliter of sample. A highly sensitive and novel GC-FID method has been developed and reported herein for the simultaneous quantification of paracetamol (PCM) and caffeine (CAF) in samples up to trace levels. The method was validated as per ICH guidelines for its sensitivity, linearity, robustness, inter and intra-day variations, limit of quantification (LOQ), limit of detection (LOD), matrix effect, carryover, precision, and accuracy. The LOD of PCM and CAF were determined to be 100 ppm and 10 ppm whereas, LOQ of PCM and CAF were found to be 300 and 30 ppm respectively. The method was applied to quantify PCM and CAF in marketed tablets and dissolution samples of the tablets, which showed highly precise and accurate quantification of PCM and CAF. Moreover, the GC-FID method was compared with reported HPLC method which suggested the superiority of GC-FID method in performance and sensitivity. In short, the newly developed GC-FID method showed sensitivity and selectivity for PCM and CAF estimation and can be adopted as an efficient method for various applications.

DEVELOPMENT AND VALIDATION OF RP HPLC METHOD FOR THE ESTIMATION OF SOFOSBUVIR IN BULK, TABLET AND INDUSTRIAL WASTE WATER

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (06) ◽  
pp. 59-66
Author(s):  
V Dhanunjayachary ◽  
◽  
V.L.S. Likhitha ◽  
Sri K. Vijaya ◽  
M. A Madhuri
Keyword(s):  
Industrial Waste ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Limit Of Quantitation ◽  
Development And Validation

The study was aimed at development and validation of RP-HPLC method for estimation of sofosbuvir in bulk, pharmaceutical dosage form and pharmaceutical industrial waste. The chromatographic separation was performed on Agilent Syncronis C 18 (100 mm × 4.6 mm, 5μm) column, with a mobile phase comprising of a mixture of methanol: acetonitrile: water (45:30:25 v/v/V). The flow rate was 1.0 mL/min with detection at 260 nm. Retention time of sofosbuvir was found to be 2.040 min. As per ICH guidelines, the method was validated for linearity, accuracy, limit of detection, limit of quantitation, precision, robustness and system suitability. Linearity was found to be in the range of 4-24 μg/mL with regression equation y = 675284.x + 49120 and correlation coefficient 0.999. The low % RSD values indicate the method to be accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.046 and 0.1400 μg/mL, respectively. The % recovery of tablets was found to be in the range of 99.9– 101.3%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for estimation of sofosbuvir in bulk, tablet and applicable for analyses of in pharmaceutical industrial waste.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

RAPID RP-HPLC METHOD DEVELOPMENT AND VALIDATION OF LURASIDONE HYHROCHLORIDE IN BULK AND TABLET FORM

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (01) ◽  
pp. 28-34
Author(s):  
K. Vijaya Sri ◽  
M. Shiva Kumar ◽  
A. Sravani ◽  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Tablet Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

The RP-HPLC were developed and validated for the estimation of lurasidone HCl as per ICH guidelines. A simple, fast, accurate and precise RP-HPLC method was developed by using methanol: water containing 0.01% ortho phosphoric acid in the ratio of 70:30 (V/V). The method was developed in Eclipse C18 column (100 mm × 4.6 mm, 3.5 μm particle size). The method was found to be linear in the range of 2.5- 15µg/mL with a correlation coefficient value of 0.999. The accuracy studies of RP-HPLC method was performed at three different levels, i.e., 50%, 100%, and 150% and recovery was found to be in the range of 100.1-100.6% .The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.30-0.92. Satisfactory validation was also obtained from recovery (99.8%) studies, intra-day and interday precision and robustness 2%. The proposed method was found to be accurate, precise and rapid for the analysis of lurasidone.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

Method Development and Validation of Spectrophotometric Methods for The Estimation of Rizatriptan Benzoate in Pure and Pharmaceutical Dosage Form

2021 ◽  
pp. 6003-6006
Author(s):  
Pushpa Latha E. ◽  
Sailaja B.
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rizatriptan Benzoate ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Analytical UV derivative spectrophotometric method was developed and validated to quantify Rizatriptan Benzoate in pure drug and tablet dosage form. Based on the spectrophotometric characteristics of Rizatriptan Benzoate, a signal of zero (225nm), first (216nm), second (237nm), third (233nm), fourth (231nm) order derivative spectra were found to be adequate for quantification. The methods obeyed Beer's law in the concentration range of (0.1-360µg/ml) with square correlation coefficient (r2) of 0.999. The mean percentage recovery was found to be 100.01 ± 0.075. As per ICH guidelines the results of the analysis were validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification, and were found to be satisfactory.

RP-HPLC METHOD FOR ESTIMATION OF LORNOXICAM IN TABLETS AND IN DISSOLUTION SAMPLES USING MASS SPECTROMETRIC COMPATIBLE BUFFERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Mass Spectrometric ◽  
Control Analysis ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Liquid Chromatographic

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.

Development and Validation of the Analytical method for the estimation of a combination of 5-fluorouracil and Imiquimod by RP-HPLC

2021 ◽  
pp. 3313-3318
Author(s):  
Bhupender Tomar ◽  
Ankita Sharma ◽  
Inder Kumar ◽  
Sandeep Jain ◽  
Pallavi Ahirrao
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Pharmaceutical Ingredients ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, precise, and accurate reverse phase high performance liquid chromatographic method (RP-HPLC) was developed and validated for the estimation of the combination of 5- Fluorouracil (5-FU) and Imiquimod in active pharmaceutical ingredients (APIs). The method was carried out on Phenomenex C18 (250 × 4.6mm I.D., 5𝜇m) using isocratic elution mode. The mobile phase was used as Acetonitrile: 10mM potassium dihydrogen orthophosphate: triethylamine (40:59.9:0.1, v/v, pH 4.5 with orthophosphoric acid) and Water: ACN (50:50 v/v) was used as a diluent. The concentration of solvents was 1-20µg/ml and the volume of injection was 20µl with the flow rate of 1.2ml/min. The retention times for 5-FU and Imiquimod were found to be 1.9±0.5 and 6.6±0.5 min respectively. The absorption maxima of 5FU and Imiquimod were found 267nm and 227nm respectively. The method was validated as per ICH guidelines. All the data were found within the specified limits. The limit of detection (LOD) and limit of quantification (LOQ) of 5- Fluorouracil were found to be 0.015μg/mL and 0.048 μg/mL, respectively, and Imiquimod was found to be 0.078μg/mL and 0.237μg/mL, respectively. The method developed in the present study was found to be sensitive, specific, and precise and can be applied for the simultaneous estimation of 5-FU and Imiquimod.

High performance liquid chromatography (HPLC) method development and validation for the determination of flunixin: Animal plasma based study

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Hplc Method Development ◽  
Development And Validation

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.

scholarly journals UPLC Method Development and Validation for the Determination of Chlophedianol Hydrochloride in Syrup Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 25-31
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Analysis Data ◽  
Calibration Plot ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation

A specific, precise, accurate ultra pressure liquid chromatography (UPLC) method is developed for estimation of chlophedianol hydrochloride in bulk drug and syrup dosage form. The method employed with Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) in a gradient mode, with mobile phase of methanol and acetonitrile in the ratio of 65:35 %v/v. The flow rate was 0.1 ml/min and effluent was monitored at 254 nm. Retention time was found to be 1.130±0.005 min. The method was validated in terms of linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ)in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was good linear relationship between response and concentration in the range of 20-100 μg/ml respectively. The LOD and LOQ values were found to be 2.094(μg/ml)and 6.3466(μg/ml)respectively. No chromatographic interference from syrup excipients and degradants were found. The proposed method was successfully used for estimation of chlophedianol hydrochloride in syrup dosage form.

A NOVEL HPLC METHOD FOR ESTIMATION OF GENOTOXIC IMPURITY 3-ACETAMIDOBENZENE 1, 2 DICARBOXYLIC ACID IN KEY STARTING MATERIAL 3-ACETAMIDOPTHALIC ANHYDRIDE OF APREMILAST API

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (05) ◽  
pp. 42-46
Author(s):  
P. Shinde ◽  
◽  
S. Shirke ◽  
R. Dwivedi ◽  
U Dhuppad
Keyword(s):  
Dicarboxylic Acid ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Research Work ◽  
Hplc Method ◽  
Starting Material ◽  
Phase Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Normal Phase Hplc

3-Acetamidobenzene -1, 2-dicarboxylic acid is a potential genotoxic impurity which gets formed during synthesis of 3- acetamidopthalic anhydride, a Key Starting Material (KSM) for manufacturing of apremilast API. During handling upon exposure to moisture, the anhydride ring of KSM 3-acetamidopthalic anhydride opens to form the acid. Hence Reverse phase HPLC method is not a feasible and robust option for estimation of this impurity. To overcome these problems a normal phase HPLC method is developed and proposed in this research work. Immobilized Chiral pack IA column from Daicel is used for estimation. n-Hexane and isopropyl alcohol in 90:10 (v/v) ratio modified with 0.1% trifluroacetic acid is used as mobile phase. Method is validated as per ICH guidelines. Limit of Detection (LOD) and Limit of Quantification (LOQ) are found to be 0.47 ppm (0.0047%) and 1.42 ppm (0.0142%), respectively. The method is linear over LOQ to 150%. Recovery is within limits (80-120%). Method is robust for parameters like mobile phase composition, flow rate, wavelength changes and column oven temperature.

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